CN103880087A - Tungsten oxide aerogel as well as preparation method and application thereof - Google Patents
Tungsten oxide aerogel as well as preparation method and application thereof Download PDFInfo
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- CN103880087A CN103880087A CN201410135464.3A CN201410135464A CN103880087A CN 103880087 A CN103880087 A CN 103880087A CN 201410135464 A CN201410135464 A CN 201410135464A CN 103880087 A CN103880087 A CN 103880087A
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Abstract
The invention discloses a preparation method of tungsten oxide aerogel. The method comprises the following steps: uniformly mixing tungstic acid and polyethylene imine in water at a mass ratio of 1:1; adjusting the pH to 1-5; adding water for diluting until the mass fractions of tungstic acid and polyethylene imine in a solution are 0.05-0.1 respectively; performing a hydrothermal reaction on an obtained mixed solution to obtain hydrogel; performing freeze drying or supercritical drying on the hydrogel to obtain the tungsten oxide aerogel. The method is a hydrothermal auxiliary gel method. Tungsten oxide growths into nanowires in an oriented way by adding polyethylene imine as a morphology guiding agent, and the nanowires are wound together into a spatial three-dimensional netlike structure, thereby constructing the tungsten oxide aerogel finally. The aerogel prepared by winding the nanowires contributes to fixing of protease, can be taken as a relay baton for use in protease direct electron transfer, contributes to the implementation of protease direction electrochemistry, and can be used for constructing a testing electrode of an efficient and stable direct electrochemical biosensor.
Description
Technical field
The invention belongs to material preparation and application technical field, relate to a kind of inorganic aerogels and its preparation method and application.
Background technology
Tungsten oxide 99.999 is a kind of novel semiconductor material, also be that a few is easy to one of oxide semiconductor of realizing quantum size effect, have the characteristics such as electrochromism, absorption, catalysis concurrently, be widely used in the fields such as photoelectric device, chemical sensor, fuel cell.In recent years due to the efficient variable color of development, metasable state of tungsten oxide nanometer material preparation technology and the discovery of transmitting proton performance, based on tungsten oxide nanometer material uv-absorbing and chemically reactive, its application expands to again multiple fields such as information storage, color-changing window, big area information display screen, auto mirror.
Aerogel is a kind ofly mutually to be assembled the nanoporous network being built into by nanometer scale ultrafine particulate or high-polymer molecular, and in space, is full of a kind of high dispersive solid-state material of gaseous state dispersion medium.Its porosity can reach 80～99.8%, and hole dimension is generally between 1～100nm, and density range can be at 3～600mg/cm
3.1931, American scientist Kistler reported first SiO
2synthesizing of aerogel, but because synthesis technique is loaded down with trivial details, consuming time, fail developed.To the seventies in last century, along with the development of sol-gel technique and the enhancing of awareness of saving energy, there is the aerogel that extremely-low density, vesicular structure, good adsorptivity and structure be easy to the advantages such as regulation and control and cause gradually people's concern, it is at lagging material, and the fields such as sound-proof material, filtering material, catalyzer, sorbent material, sensor, fuel cell, particle detector, Thermosensitive Material Used for Controlled Releasing of Medicine all demonstrate advantageous advantage.The preparation of inorganic aerogels generally selects metallorganics (also having a small amount of nonmetal as the organism of Si, B etc.) as raw material, first utilize sol-gel process in solution, to form colloidal solid unordered, dendritic, contiguous network structure, adopt again supercritical drying drying process to remove remaining solution in gel and do not change the structure of gel state, obtaining thus porous, unordered, the low density amorphous solid-state material with nanometer scale contiguous network structure.At present, application sol-gel method and supercritical drying drying process have been prepared SiO
2, Al
2o
3and TiO
2deng tens kinds of aerogels.
Biosensor is to use biological active materials as sensor, utilizes physics transverter biochemical reaction can be converted to the analysis test apparatus of physicochemical change signal.Its analytical procedure is the advanced detecting & monitoring method of the development requisite one of biotechnology, is also quick, the trace analysis method of material molecule level.In following 21 century knowledge economy development; biosensor technique will be the new growing point between information and biotechnology, in the researchs such as clinical diagnosis, Industry Control, food and pharmaceutical analysis, environment protection and biotechnology and biochip, has a wide range of applications.Protein (enzyme) is the immobilization biological function reagent being most widely used in electrochemica biological sensor, for the preparation of sensor sensing film, can realize highly selective and the highly sensitive detection of sensor to substrate.In theory, direct electron transfer between protein (enzyme) and electrode for good, the highly sensitive biosensor of design alternative provide may, but since Clark in 1962 proposes the concept of biosensor, up to now, only have minority redox protein (enzyme) on naked solid electrode, to show electrochemical activity, want to realize the direct electron transfer not a duck soup between redox protein (enzyme) and electrode.In recent years, due to medialess Direct Electrochemistry biosensor have highly sensitive, selectivity good, immunity from interference is strong, be easy to the advantage such as microminiaturization and automatization, caused the research interest that scientists is strong.But want really to realize the practical of Direct Electrochemistry type biosensor, the efficient stable maintenance of necessary assurance zymoprotein catalytic activity and zymoprotein reaction signal are to effective transmission of signal conversion element, and these two conditions are indispensable.Inorganic aerogels is because porosity own is high, and pore structure is distributed as intermediary hole structure, has again larger specific surface area, provides possibility for building the Direct Electrochemistry biological sensor electrode of efficient stable.TiO
2, SiO
2all once for modified biological sensor electrode, but the application in biosensor there is not yet bibliographical information about Tungsten oxide 99.999 aerogel with graphene aerogel etc.
Summary of the invention
In view of this, one of object of the present invention is to provide a kind of preparation method of Tungsten oxide 99.999 aerogel, and reaction is simple, with low cost, gained; Two of object is to provide the application of the employing Tungsten oxide 99.999 aerogel that described method makes in electrochemica biological sensor.
After deliberation, the invention provides following technical scheme:
1. the preparation method of Tungsten oxide 99.999 aerogel, that wolframic acid is mixed in water for 1:1 in mass ratio with polymine, regulate pH to 1-5, be diluted with water to the massfraction of wolframic acid and polymine in solution and be respectively 0.05～0.1, gained mixed solution makes hydrogel by hydro-thermal reaction, again hydrogel is carried out to lyophilize or supercritical drying, make Tungsten oxide 99.999 aerogel.
The present invention can be directly with wolframic acid as tungsten source, but because wolframic acid is unstable, see that light easily decomposes, often now with the current in practical application, use tungstate (as sodium wolframate etc.) to make with mineral acid (example hydrochloric acid, sulfuric acid etc.) hybrid reaction.
Further, described wolframic acid adopts following methods to make: by the mineral acid acidifying of the tungstate aqueous solution, separate out wolframic acid precipitation, and solid-liquid separation, solid, after washing, be dried, pulverize, obtains wolframic acid powder.
Further, described tungstate is sodium wolframate, and described mineral acid is hydrochloric acid or sulfuric acid.
Further, described hydro-thermal reaction is reacting by heating 18～30 hours under 180 ℃～210 ℃ conditions.
Further, the preparation method of described Tungsten oxide 99.999 aerogel mixes for 1:1 wolframic acid in mass ratio with polymine in water, with salt acid for adjusting pH to 3, be diluted with water to the massfraction of wolframic acid and polymine in solution and be respectively 0.07, gained mixed solution makes hydrogel for 24 hours in 210 ℃ of reacting by heating, again hydrogel is carried out to lyophilize, make Tungsten oxide 99.999 aerogel.
2. the Tungsten oxide 99.999 aerogel that adopts above-mentioned preparation method to make.
3. the application of Tungsten oxide 99.999 aerogel in preparation Direct Electrochemistry type biosensor test electrode described in.
4. utilize described Tungsten oxide 99.999 aerogel to prepare the method for Direct Electrochemistry type biosensor test electrode, comprise the following steps:
A. get Tungsten oxide 99.999 aerogel, add water, ultrasonic dispersion, adds proteolytic enzyme, and concussion mixes, and 2～8 ℃ of placements make the abundant adhesion protein enzyme of Tungsten oxide 99.999 aerogel for 24～72 hours, obtain mixed solution;
B. glass-carbon electrode is polished flat, after light, cleaning, drying, drip mixed solution prepared by step a at electrode surface, drying and forming-film, then drip Nafion solution on film surface is dry, makes Direct Electrochemistry type biosensor test electrode.
Further, utilize Tungsten oxide 99.999 aerogel to prepare the method for Direct Electrochemistry type glucose sensor test electrode, comprise the following steps:
A. get Tungsten oxide 99.999 aerogel, adding water to concentration is 5～20mg/mL, ultrasonic dispersion, then to add glucose oxidase be 5～20mg/mL to concentration, and concussion mixes, and 2～8 ℃ of placements make Tungsten oxide 99.999 aerogel fully adsorb glucose oxidase for 48 hours, obtain mixed solution;
B. glass-carbon electrode is polished to surfacing, light, cleaning, drying step by step with aluminium powder, drip mixed solution prepared by step a at electrode surface, drying and forming-film, then drip on film surface the Nafion solution that massfraction is 0.5%, dry, make Direct Electrochemistry type glucose sensor test electrode.
Further, utilize Tungsten oxide 99.999 aerogel to prepare the method for Direct Electrochemistry type glucose sensor test electrode, comprise the following steps:
A. get Tungsten oxide 99.999 aerogel, adding water to concentration is 10mg/mL, ultrasonic dispersion, then to add glucose oxidase to concentration be 10mg/mL, shakes 20 minutes, 4 ℃ of placements make Tungsten oxide 99.999 aerogel fully adsorb glucose oxidase for 48 hours, obtain mixed solution;
B. glass-carbon electrode is polished to surfacing, light with the aluminium powder of 0.5 μ m and 0.03 μ m successively, clean, dry, drip mixed solution 5 μ L prepared by step a at electrode surface, drying and forming-film, drip on film surface the Nafion solution 10 μ L that massfraction is 0.5% again, dry, make Direct Electrochemistry type glucose sensor test electrode.
Beneficial effect of the present invention is: the present invention utilizes hydro-thermal to assist gel method, by adding polymine as pattern directed agents, successfully make Tungsten oxide 99.999 oriented growth become nano wire, and be mutually wound around between nano wire, the continuous reticulated structure that forms space multistory, has finally formed Tungsten oxide 99.999 aerogel.This aerogel being entwined by nano wire is conducive to ankyrin enzyme, can be used as the relay baton of proteolytic enzyme Direct electron transfer, be beneficial to the realization of proteolytic enzyme Direct Electrochemistry, can be used for building the Direct Electrochemistry type biosensor test electrode of efficient stable, in electrochromism, photochemical catalysis, the aspects such as gas sensor have important using value.
Accompanying drawing explanation
In order to make object of the present invention, technical scheme and beneficial effect clearer, the invention provides following accompanying drawing and describe:
Fig. 1 is the optical photograph of the Tungsten oxide 99.999 aerogel that makes of the embodiment of the present invention 1.
Fig. 2 is X-ray diffraction (XRD) figure of the Tungsten oxide 99.999 aerogel that makes of the embodiment of the present invention 1.
Fig. 3 is embodiment of the present invention 1(a), embodiment 2(b), embodiment 3(c) scanning electronic microscope (SEM) figure of the Tungsten oxide 99.999 aerogel that makes.
Fig. 4 is embodiment of the present invention 1(a), embodiment 2(b), embodiment 3(c) transmission electron microscope (TEM) figure of the Tungsten oxide 99.999 aerogel that makes.
Fig. 5 is cyclic voltammetry curve (a) and the electric current-time curve (b) of the glucose sensor that assembles of the Tungsten oxide 99.999 aerogel that makes by the embodiment of the present invention 1.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
The preparation of embodiment 1, Tungsten oxide 99.999 aerogel
Comprise the following steps:
A. under agitation condition, by excessive 6mol/L hydrochloric acid soln acidifying for the 0.4mol/L sodium wolframate aqueous solution, separate out yellow wolframic acid precipitation, vacuum filtration, solid, through washing, 50 ℃ of dry, grindings, obtains wolframic acid powder;
B. in 20mL water, add 2.5g wolframic acid powder and 2.5g polymine, mix, with salt acid for adjusting pH to 3, add water and be settled to 35mL, be transferred in reactor, 210 ℃ of reacting by heating make hydrogel for 24 hours, by hydrogel lyophilize, make blue Tungsten oxide 99.999 aerogel again.
The preparation of embodiment 2, Tungsten oxide 99.999 aerogel
Comprise the following steps:
A. under agitation condition, by excessive 6mol/L hydrochloric acid soln acidifying for the 0.4mol/L sodium wolframate aqueous solution, separate out yellow wolframic acid precipitation, vacuum filtration, solid, through washing, 50 ℃ of dry, grindings, obtains wolframic acid powder;
B. in 20mL water, add 2.5g wolframic acid powder and 2.5g polymine, mix, with salt acid for adjusting pH to 1, add water and be settled to 35mL, be transferred in reactor, 180 ℃ of reacting by heating make hydrogel for 24 hours, by hydrogel lyophilize, make blue Tungsten oxide 99.999 aerogel again.
The preparation of embodiment 3, Tungsten oxide 99.999 aerogel
Comprise the following steps:
A. under agitation condition, by excessive 6mol/L hydrochloric acid soln acidifying for the 0.4mol/L sodium wolframate aqueous solution, separate out yellow wolframic acid precipitation, vacuum filtration, solid, through washing, 50 ℃ of dry, grindings, obtains wolframic acid powder;
B. in 20mL water, add 2g wolframic acid powder and 2g polymine, mix, with salt acid for adjusting pH to 1, add water and be settled to 35mL, be transferred in reactor, 210 ℃ of reacting by heating make hydrogel for 24 hours, by hydrogel lyophilize, make blue Tungsten oxide 99.999 aerogel again.
Fig. 1 is the optical photograph of the Tungsten oxide 99.999 aerogel prepared of embodiment 1, and products therefrom is blue cylinder.
Fig. 2 is the XRD figure of the Tungsten oxide 99.999 aerogel prepared of embodiment 1.As shown in the figure, the XRD peak value of gained Tungsten oxide 99.999 aerogel is stronger, illustrates that it has good degree of crystallinity; By contrasting with standard diagram, confirm that its molecular formula is W
18o
49.
The pH value of reacting in step b can regulate in 1～5 scope, the slightly difference of product microscopic appearance that different pH values obtain.Fig. 3 is embodiment 1(a), embodiment 2(b), embodiment 3(c) the SEM figure of the Tungsten oxide 99.999 aerogel that makes.As shown in the figure, embodiment 1 gained Tungsten oxide 99.999 aerogel is made up of the nano wire of elongated (diameter 10 nanometers), has staggered tridimensional network; The nano wire of embodiment 2 gained Tungsten oxide 99.999 aerogels becomes shorter, and is not the nano wire of complete moulding; In nano wire, also there is nanometer rod in embodiment 3 gained Tungsten oxide 99.999 aerogels.Fig. 4 a is embodiment 1(a), embodiment 2(b), embodiment 3(c) the TEM figure of the Tungsten oxide 99.999 aerogel that makes, its result and SEM result fit like a glove.
The preparation of the Direct Electrochemistry type glucose sensor test electrode that embodiment 4, Tungsten oxide 99.999 aerogel are modified
Comprise the following steps:
A. get Tungsten oxide 99.999 aerogel prepared by embodiment 1, adding water to concentration is 10mg/mL, ultrasonic dispersion, adding glucose oxidase to concentration is 10mg/mL again, shake 20 minutes, 4 ℃ of placements make Tungsten oxide 99.999 aerogel fully adsorb glucose oxidase for 48 hours, obtain mixed solution;
B. by glass-carbon electrode successively with the aluminium powder of 0.5 μ m and 0.03 μ m polish flat, after light, clean, dry, drip mixed solution 5 μ L prepared by step a at electrode surface, dry film forming, drip on film surface the Nafion solution 10 μ L that massfraction is 0.5% again, dry, make the Direct Electrochemistry type glucose sensor test electrode that Tungsten oxide 99.999 aerogel is modified.
The Direct Electrochemistry type glucose sensor test electrode that Tungsten oxide 99.999 aerogel prepared by the present embodiment is modified is for glucose detection analysis.Fig. 5 is cyclic voltammetry curve (a) and the electric current-time curve (b) of the glucose sensor that assembles of the Tungsten oxide 99.999 aerogel that makes by the embodiment of the present invention 1.Cyclic voltammetry is to carry out in the PBS of 10ml0.01mol/L, pH7.0 buffered soln.Can find out from cyclic voltammetry curve,, all there is not redox peak in the electrode of being made up of independent Tungsten oxide 99.999 aerogel and the electrode of being made up of independent glucose oxidase; And the electrode that has the Tungsten oxide 99.999 aerogel of glucose oxidase to make with absorption has occurred obvious redox peak at about-0.4 volt, confirm the Direct Electrochemistry performance of glucose oxidase on Tungsten oxide 99.999 aerogel material.Can find out from electric current-time curve, after the every rising 0.1mmol/L of glucose concn, electric current has obvious response, illustrates with adsorbing the electrode pair glucose that has the Tungsten oxide 99.999 aerogel of glucose oxidase to make and has good detection performance.
Finally explanation is, above preferred embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is described in detail by above preferred embodiment, but those skilled in the art are to be understood that, can make various changes to it in the form and details, and not depart from the claims in the present invention book limited range.
Claims (10)
1. the preparation method of Tungsten oxide 99.999 aerogel, it is characterized in that, wolframic acid is mixed in water for 1:1 in mass ratio with polymine, regulate pH to 1-5, be diluted with water to the massfraction of wolframic acid and polymine in solution and be respectively 0.05～0.1, gained mixed solution makes hydrogel by hydro-thermal reaction, then hydrogel is carried out to lyophilize or supercritical drying, makes Tungsten oxide 99.999 aerogel.
2. the preparation method of Tungsten oxide 99.999 aerogel as claimed in claim 1, is characterized in that, described wolframic acid adopts following methods to make: by the mineral acid acidifying of the tungstate aqueous solution, separate out wolframic acid precipitation, solid-liquid separation, solid, after washing, be dried, pulverize, obtains wolframic acid powder.
3. the preparation method of Tungsten oxide 99.999 aerogel as claimed in claim 2, is characterized in that, described tungstate is sodium wolframate, and described mineral acid is hydrochloric acid or sulfuric acid.
4. the preparation method of Tungsten oxide 99.999 aerogel as claimed in claim 1, is characterized in that, described hydro-thermal reaction is reacting by heating 18～30 hours under 180 ℃～210 ℃ conditions.
5. the preparation method of the Tungsten oxide 99.999 aerogel as described in claim 1 to 4 any one, it is characterized in that, wolframic acid is mixed in water for 1:1 in mass ratio with polymine, with salt acid for adjusting pH to 3, be diluted with water to the massfraction of wolframic acid and polymine in solution and be respectively 0.07, gained mixed solution makes hydrogel for 24 hours in 210 ℃ of reacting by heating, then hydrogel is carried out to lyophilize, makes Tungsten oxide 99.999 aerogel.
6. the Tungsten oxide 99.999 aerogel that described in employing claim 1 to 5 any one, preparation method makes.
7. the application of Tungsten oxide 99.999 aerogel in preparation Direct Electrochemistry type biosensor test electrode described in claim 6.
8. utilize Tungsten oxide 99.999 aerogel described in claim 6 to prepare the method for Direct Electrochemistry type biosensor test electrode, it is characterized in that, comprise the following steps:
A. get Tungsten oxide 99.999 aerogel, add water, ultrasonic dispersion, adds proteolytic enzyme, and concussion mixes, and places 24～72 hours for 2～8 ℃, makes the abundant adhesion protein enzyme of Tungsten oxide 99.999 aerogel, obtains mixed solution;
B. glass-carbon electrode is polished flat, after light, cleaning, drying, drip mixed solution prepared by step a at electrode surface, drying and forming-film, then drip Nafion solution on film surface is dry, makes Direct Electrochemistry type biosensor test electrode.
9. utilize as claimed in claim 8 Tungsten oxide 99.999 aerogel to prepare the method for Direct Electrochemistry type biosensor test electrode, it is characterized in that, comprise the following steps:
A. get Tungsten oxide 99.999 aerogel, adding water to concentration is 5～20mg/mL, ultrasonic dispersion, then to add glucose oxidase be 5～20mg/mL to concentration, and concussion mixes, and 2～8 ℃ of placements make Tungsten oxide 99.999 aerogel fully adsorb glucose oxidase for 48 hours, obtain mixed solution;
B. glass-carbon electrode is polished to surfacing, light, cleaning, drying step by step with aluminium powder, drip mixed solution prepared by step a at electrode surface, drying and forming-film, then drip on film surface the Nafion solution that massfraction is 0.5%, dry, make Direct Electrochemistry type glucose sensor test electrode.
10. utilize as claimed in claim 9 Tungsten oxide 99.999 aerogel to prepare the method for Direct Electrochemistry type biosensor test electrode, it is characterized in that, comprise the following steps:
A. get Tungsten oxide 99.999 aerogel, adding water to concentration is 10mg/mL, ultrasonic dispersion, then to add glucose oxidase to concentration be 10mg/mL, shakes 20 minutes, 4 ℃ of placements make Tungsten oxide 99.999 aerogel fully adsorb glucose oxidase for 48 hours, obtain mixed solution;
B. glass-carbon electrode is polished to surfacing, light with the aluminium powder of 0.5 μ m and 0.03 μ m successively, clean, dry, drip mixed solution 5 μ L prepared by step a at electrode surface, drying and forming-film, drip on film surface the Nafion solution 10 μ L that massfraction is 0.5% again, dry, make Direct Electrochemistry type glucose sensor test electrode.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104730115A (en) * | 2015-02-09 | 2015-06-24 | 西南大学 | Novel biological and gas sensor based on bionic honeycomb coal aerogel material |
| CN108946815A (en) * | 2018-08-23 | 2018-12-07 | 东北大学 | A kind of WO3Nano particle and preparation method and its application in the sensor |
| CN109987634A (en) * | 2017-12-30 | 2019-07-09 | 卢斌 | A kind of WO3The preparation method of aeroge |
| CN113235130A (en) * | 2021-04-12 | 2021-08-10 | 中山大学 | Low-platinum composite material based on tungsten oxide/graphene aerogel and preparation method and application thereof |
| CN114229897A (en) * | 2021-09-14 | 2022-03-25 | 中国科学技术大学 | Preparation method of metal phase tungsten oxide and application of metal phase tungsten oxide |
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| CN102070195A (en) * | 2010-12-20 | 2011-05-25 | 大连工业大学 | Mesoporous WO3 aerogel and preparation method thereof |
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| CN102070195A (en) * | 2010-12-20 | 2011-05-25 | 大连工业大学 | Mesoporous WO3 aerogel and preparation method thereof |
| CN103407997A (en) * | 2013-07-19 | 2013-11-27 | 北京航空航天大学 | Macro preparation method of macroscopic three-dimensional graphene aerogel adsorption material used for indoor air purification |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104730115A (en) * | 2015-02-09 | 2015-06-24 | 西南大学 | Novel biological and gas sensor based on bionic honeycomb coal aerogel material |
| CN109987634A (en) * | 2017-12-30 | 2019-07-09 | 卢斌 | A kind of WO3The preparation method of aeroge |
| CN108946815A (en) * | 2018-08-23 | 2018-12-07 | 东北大学 | A kind of WO3Nano particle and preparation method and its application in the sensor |
| CN113235130A (en) * | 2021-04-12 | 2021-08-10 | 中山大学 | Low-platinum composite material based on tungsten oxide/graphene aerogel and preparation method and application thereof |
| CN114229897A (en) * | 2021-09-14 | 2022-03-25 | 中国科学技术大学 | Preparation method of metal phase tungsten oxide and application of metal phase tungsten oxide |
| CN114229897B (en) * | 2021-09-14 | 2022-09-30 | 中国科学技术大学 | Preparation method of metal phase tungsten oxide and application of metal phase tungsten oxide |
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